US8715390B2 - Method of separating off trace components from a fraction containing at least nitrogen and helium - Google Patents
Method of separating off trace components from a fraction containing at least nitrogen and helium Download PDFInfo
- Publication number
- US8715390B2 US8715390B2 US13/367,484 US201213367484A US8715390B2 US 8715390 B2 US8715390 B2 US 8715390B2 US 201213367484 A US201213367484 A US 201213367484A US 8715390 B2 US8715390 B2 US 8715390B2
- Authority
- US
- United States
- Prior art keywords
- fraction
- helium
- nitrogen
- separation column
- trace components
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related, expires
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Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
- F25J3/028—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of noble gases
- F25J3/029—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of noble gases of helium
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/0204—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the feed stream
- F25J3/0209—Natural gas or substitute natural gas
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
- F25J3/0233—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of CnHm with 1 carbon atom or more
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
- F25J3/0257—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of nitrogen
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/08—Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/02—Processes or apparatus using separation by rectification in a single pressure main column system
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/90—Details relating to column internals, e.g. structured packing, gas or liquid distribution
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2205/00—Processes or apparatus using other separation and/or other processing means
- F25J2205/02—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum
- F25J2205/04—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum in the feed line, i.e. upstream of the fractionation step
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2205/00—Processes or apparatus using other separation and/or other processing means
- F25J2205/30—Processes or apparatus using other separation and/or other processing means using a washing, e.g. "scrubbing" or bubble column for purification purposes
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2210/00—Processes characterised by the type or other details of the feed stream
- F25J2210/42—Nitrogen
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2215/00—Processes characterised by the type or other details of the product stream
- F25J2215/30—Helium
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2270/00—Refrigeration techniques used
- F25J2270/90—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration
- F25J2270/904—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration by liquid or gaseous cryogen in an open loop
Definitions
- the invention relates to a method for separating off trace components from a fraction containing at least nitrogen and helium, wherein this fraction is partially condensed for the enrichment of the helium.
- Methods of the type in question for separating off trace components from a fraction containing at least nitrogen and helium are used, for example, in the recovery of helium from natural gas.
- the typical concentrations of these trace components are, for example, up to 5% methane, up to 0.5% ethane, up to 0.5% ethylene, up to 0.1% oxygen, up to 0.5% argon, and up to 0.1% hydrogen.
- the fraction containing at least nitrogen and helium is usually, during the cooling and liquefaction process of a natural gas stream, separated off therefrom and processed to form a helium-enriched stream which, in the present case, is the desired product stream.
- Separating off nitrogen and optionally other components such as, for example, methane, oxygen etc., from the fraction containing at least nitrogen and helium usually proceeds after partial condensation in a separator vessel or separator. Separation of the individual components of the fraction containing at least nitrogen or helium proceeds in accordance with the thermodynamic equilibrium at the prevailing temperature and the prevailing pressure of the mixture.
- the gas phase taken off at the top of the separator can comprise a comparatively high residual contamination of methane, oxygen, etc.
- a liquid nitrogen fraction (LIN) is taken off as product.
- LIN liquid nitrogen fraction
- a method of the type in question for separating off trace components from a fraction containing at least nitrogen and helium which is characterized in that the partially condensed fraction is fed at least in part to at least one separation column and separated therein into a helium-rich gas fraction and a nitrogen-rich liquid fraction which contains the trace components.
- the helium-rich gas can contain less than 0.5% methane, up to 0.1% oxygen, and up to 0.1% argon.
- the separation of the fraction containing at least nitrogen and helium into a helium-enriched gas fraction and a nitrogen-rich liquid fraction proceeds in at least one separation column, wherein the abovementioned fraction is fed to the separation column in the bottom region, preferably in the sump of the separation column.
- the separation column is provided with a plurality of bubble-cap trays and/or ordered or structured packings, whereby the effectiveness of the separation process proceeding therein is increased.
- a cold reflux medium is fed to the separation column top and distributed therein.
- FIGURE illustrates an exemplary embodiment of the invention.
- a separator D is connected upstream of the separation column T that is to be provided according to the invention.
- This separator can alternatively be integrated in the lower part of the separation column, preferably in the bottom part thereof.
- the fraction 1 containing at least nitrogen and helium that is to be separated contains only a few percent of methane and helium and optionally a few parts per thousand of oxygen, argon and hydrogen, and the remainder is nitrogen.
- This fraction has a temperature of above 300 K and is cooled to a temperature of approximately 80 K in the heat exchanger E in countercurrent to process streams which are to be warmed, and which will be considered in more detail hereinafter.
- the cooled fraction is fed via line 2 to the separator D.
- a first nitrogen-rich fraction is taken off via line 3 and cold-producingly expanded in the expansion valve a.
- the first nitrogen-rich fraction is enriched with regards to the concentrations of methane and oxygen.
- a helium-enriched fraction is taken off via line 4 and delivered to the separation column T in the lower region thereof.
- a plurality of ordered packings and/or bubble-cap trays are arranged within the separation column T for the purpose of increasing the efficacy of the separation process.
- a cold reflux medium is fed to the top of the separation column T; this is preferably liquid nitrogen or a nitrogen-rich liquid fraction.
- a second nitrogen-rich fraction is taken off from the bottom phase of the separation column T via line 5 , cold-producingly expanded in the valve b and combined with the first nitrogen-rich fraction 3 to form stream 8 .
- This stream is warmed in the heat exchanger E against the feed fraction 1 that is to be cooled and then, via line 9 , or preferably after combustion of the methane, delivered to the atmosphere.
- the second nitrogen-rich fraction is enriched with regards to the concentrations of methane and oxygen.
- a nitrogen- and helium-rich fraction 6 is taken off.
- the methane, oxygen and hydrogen content thereof are in the parts per thousand range, whereas it comprises helium in accordance with the content in the feed fraction 1 .
- the fraction 6 in the heat exchanger E, is likewise warmed against the feed fraction 1 that is to be cooled and fed via line 7 to further use thereof, for example in a further enrichment and liquefaction of the helium which are not shown in the figure.
- the method according to the invention for separating off trace components from a fraction containing at least nitrogen and helium is a more effective separation and purification method, compared with the known prior art and, furthermore, saves energy and also costs.
- the amount of reflux medium or additional liquid nitrogen for the reflux 10 of the separation column T can be adapted to the respective feed conditions, from which a considerable saving in operating costs results.
- the operating costs of the separation column to be provided according to the invention are not higher. Complex post-purification processes required to date can now be simplified or even dispensed with.
- the abovementioned components methane and oxygen are separated off together with the nitrogen as bottom phase product of the separation column T. If the nitrogen-rich fraction(s) obtained from the overhead product of the separation column T is (are) to be liquefied and used, for example, within the further process as cooling medium, attention must be paid to the fact that, owing to the concentration of methane and/or oxygen, an explosive or combustible gas mixture can be formed.
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- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Mechanical Engineering (AREA)
- Thermal Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Separation By Low-Temperature Treatments (AREA)
Abstract
Description
-
- the partially condensed fraction is first fed to a separator and the helium-enriched gas fraction obtained from the separator is fed at least in part to the at least one separation column,
- nitrogen or a nitrogen-rich fraction as reflux medium is fed to the separation column, and
- the separation task within the separation column is supported by ordered packings and/or bubble-cap trays arranged therein.
Claims (10)
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102011010634 | 2011-02-08 | ||
DE102011010634.0 | 2011-02-08 | ||
DE102011010634A DE102011010634A1 (en) | 2011-02-08 | 2011-02-08 | A method of separating trace components from a fraction containing at least nitrogen and helium |
Publications (2)
Publication Number | Publication Date |
---|---|
US20120198997A1 US20120198997A1 (en) | 2012-08-09 |
US8715390B2 true US8715390B2 (en) | 2014-05-06 |
Family
ID=46547035
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US13/367,484 Expired - Fee Related US8715390B2 (en) | 2011-02-08 | 2012-02-07 | Method of separating off trace components from a fraction containing at least nitrogen and helium |
Country Status (4)
Country | Link |
---|---|
US (1) | US8715390B2 (en) |
AU (1) | AU2012200384B2 (en) |
DE (1) | DE102011010634A1 (en) |
RU (1) | RU2579792C2 (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US11686528B2 (en) | 2019-04-23 | 2023-06-27 | Chart Energy & Chemicals, Inc. | Single column nitrogen rejection unit with side draw heat pump reflux system and method |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102013007208A1 (en) | 2013-04-25 | 2014-10-30 | Linde Aktiengesellschaft | Process for recovering a methane-rich liquid fraction |
DE102015001664A1 (en) * | 2015-02-10 | 2016-08-11 | Linde Aktiengesellschaft | Helium recovery process |
US11079176B2 (en) | 2018-03-14 | 2021-08-03 | Exxonmobil Upstream Research Company | Method and system for liquefaction of natural gas using liquid nitrogen |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5771714A (en) * | 1997-08-01 | 1998-06-30 | Praxair Technology, Inc. | Cryogenic rectification system for producing higher purity helium |
US20090013718A1 (en) * | 2005-03-04 | 2009-01-15 | Linde Aktiengesellschaft | Method for the simultaneous recovery of a pure helium and pure nitrogen fraction |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE10106484A1 (en) * | 2001-02-13 | 2002-08-14 | Linde Ag | Simultaneous recovery of helium and nitrogen pure fractions from process stream containing methane, nitrogen and helium, involves partially condensing process stream, and further processing |
US7437889B2 (en) * | 2006-01-11 | 2008-10-21 | Air Products And Chemicals, Inc. | Method and apparatus for producing products from natural gas including helium and liquefied natural gas |
-
2011
- 2011-02-08 DE DE102011010634A patent/DE102011010634A1/en not_active Ceased
-
2012
- 2012-01-23 AU AU2012200384A patent/AU2012200384B2/en active Active
- 2012-02-07 RU RU2012104231/06A patent/RU2579792C2/en active
- 2012-02-07 US US13/367,484 patent/US8715390B2/en not_active Expired - Fee Related
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5771714A (en) * | 1997-08-01 | 1998-06-30 | Praxair Technology, Inc. | Cryogenic rectification system for producing higher purity helium |
US20090013718A1 (en) * | 2005-03-04 | 2009-01-15 | Linde Aktiengesellschaft | Method for the simultaneous recovery of a pure helium and pure nitrogen fraction |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US11686528B2 (en) | 2019-04-23 | 2023-06-27 | Chart Energy & Chemicals, Inc. | Single column nitrogen rejection unit with side draw heat pump reflux system and method |
Also Published As
Publication number | Publication date |
---|---|
US20120198997A1 (en) | 2012-08-09 |
RU2012104231A (en) | 2013-08-20 |
RU2579792C2 (en) | 2016-04-10 |
AU2012200384A1 (en) | 2012-08-23 |
DE102011010634A1 (en) | 2012-08-09 |
AU2012200384B2 (en) | 2014-11-06 |
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